CN106525710A - Electrochemical testing device for acoustic-emission-testing-material corrosion performance and application method thereof - Google Patents
Electrochemical testing device for acoustic-emission-testing-material corrosion performance and application method thereof Download PDFInfo
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- CN106525710A CN106525710A CN201611178470.2A CN201611178470A CN106525710A CN 106525710 A CN106525710 A CN 106525710A CN 201611178470 A CN201611178470 A CN 201611178470A CN 106525710 A CN106525710 A CN 106525710A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/14—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object using acoustic emission techniques
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses an electrochemical testing device for the acoustic-emission-testing-material corrosion performance and an application method thereof. The electrochemical testing device comprises an electrolytic tank, an electrochemical testing device, a heating device and a heat preservation device. The electrolytic tank comprises a reaction tank, a reaction tank cover, a sealing gasket, fastening devices and a sample installing device; the sample installing device is composed of a stepped screw wave-guiding rod, a primary sleeve, a secondary sleeve, a tertiary sleeve, a sealing ring and an acoustic emission sensor; the electrochemical testing device comprises an auxiliary electrode clamp, a reference electrode clamp, a working electrode clamp and an electrochemical data processing system, an auxiliary electrode is a platinum net electrode, a reference electrode is installed in a luggin capillary, the heating device is arranged on the outer side of the reaction tank, and the heat preservation device is arranged on the outer side of the heating device. According to the electrochemical testing device for the acoustic-emission-testing-material corrosion performance and the application method thereof, the acoustic emission dynamic nondestructive testing technology and the electrochemical testing technology are integrated, and online, dynamic and real-time testing of the electrochemical corrosion process of a material is achieved.
Description
Technical field
The present invention relates to material corrosion performance test device field, and in particular to a kind of acoustic emission detection material corrosion performance
Electrochemical testing device and its using method.
Background technology
Corrosion is a kind of slow damage process that material occurs in harsh Service Environment, with extremely strong disguised, idol
So property, it is sudden and serious destructive the features such as.Electrochemistry is a kind of conventional Fast Evaluation material corrosion resistance
Method of testing, such as potentiodynamic polarization, constant potential polarization, circulation potentiodynamic polarization, electrochemical impedance test etc..Electrochemical techniques master
The destructive detection of small sample is directed to, it is therefore intended that prior prediction corrosion proof to material or after-action review, but cannot to
Labour large-scale component corrosion condition carries out on-line checking.Acoustic emission is a kind of highly sensitive online Dynamic Non-Destruction Measurement.With
The related passivating film cracking of corrosion, bubbles burst, stress corrosion cracking etc. are typical acoustic emission sources.Current acoustic emission is
It is successfully applied to the fields such as remote conveying oil-piping leak detection, Corrosion of Tanks degree online evaluation.But during corrosion damage
The application study of sound emission mechanism harmony transmitting qualitative assessment extent of corrosion is still within the starting stage.Sound is adopted while existing
Lift-off technology and electrochemical techniques detect that the major defect of the test device of material corrosion performance is:(1) traditional test device
The tested sample size of requirement is too big, it is impossible to carry out the test of tiny sample.While tested sample is contacted with corrosive medium also
Requirement has enough areas with waveguide rod or directly with acoustic emission sensor is connected, and this requires that the size of tested sample must set
That what is counted is sufficiently large.Welding point is typically structural member link the weakest, if it is desired to the zones of different (weldering of Welded Joints
Seam root, capping, Weld pipe mill, high temperature and low temperature heat affecting etc.) sound emission and Electrochemical Detection are carried out, the limit based on sampling
System, existing test device cannot be realized;(2) for the ease of the installation of acoustic emission sensor, tested sample is used as work
Electrode is usually required to be mounted at the bottom of electrolytic cell, therefore existing test device limits the heating to corrosive medium and guarantor
Temperature;(3) acoustic emission detection and Electrochemical Detection of material corrosion performance under various mixed gases environment cannot be simulated;(4) sample
The complex operation of installation and removal.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of specimen holder for electrochemical corrosion test
Tool and its using method;
The present invention also aims to provide a kind of fixture and its using method of acoustic emission detection material corrosion performance;
Another object of the present invention also resides in a kind of corrosion electrochemical test system of offer and its using method;
Another object of the present invention also resides in the electro-chemical test dress for providing a kind of acoustic emission detection material corrosion performance
Put and its using method.
For the sample clamp of electrochemical corrosion test, by ladder screw thread waveguide rod, one-level sleeve, two-level sleeve, three-level
Sleeve and sealing ring composition, ladder screw thread waveguide rod, one-level sleeve, two-level sleeve, three-level sleeve and sealing ring are coaxially disposed, its
In:Ladder screw thread waveguide rod is provided with the first external screw thread, the second external screw thread, and the first external screw thread is connected with the internal thread of one-level sleeve,
So that the front end of ladder screw thread waveguide rod is placed in first cavity and the second cavity of one-level sleeve, the second external screw thread is placed in one-level
On the outside of second cavity of sleeve;In the rear end of ladder screw thread waveguide rod, fixing end is set;One-level sleeve external screw thread and three-level sleeve
Internal thread is connected, so that one-level sleeve is placed in the 3rd cavity and the 4th cavity of three-level sleeve;Two-level sleeve is sleeved on three-level
On the outside of sleeve, sealing ring is set between two-level sleeve and three-level sleeve.
In above-mentioned technical proposal, the sealing ring is rubber seal.
In above-mentioned technical proposal, a diameter of 5 ± 0.01mm of the test surfaces of sample, length are 7~8mm.
In above-mentioned technical proposal, ladder screw thread waveguide rod be metal material, such as ferritic stainless steel.
In above-mentioned technical proposal, one-level sleeve, two-level sleeve, three-level sleeve are insulating materials, such as polytetrafluoroethyl-ne
Alkene.
When being used, ladder screw thread the second external screw thread of waveguide rod is connected with the internal thread of sample, in the circumference of sample
Face arranges coupling oxidant layer, rotates the fixing end of ladder screw thread waveguide rod, so as to be connected with ladder screw thread the second external screw thread of waveguide rod
Sample test surfaces, it is concordant with the second alignment surface of the first alignment surface of one-level sleeve, three-level sleeve;Using second sleeve
Internal thread is fixedly linked with test device, and carries out electrochemical corrosion test to sample, with sample as working electrode, using wire
It is connected with the ladder screw thread waveguide rod on the outside of test device, to gather the electrochemical corrosion signal on sample.
The fixture of acoustic emission detection material corrosion performance, by ladder screw thread waveguide rod, one-level sleeve, two-level sleeve, three-level
Sleeve, sealing ring and acoustic emission sensor composition, ladder screw thread waveguide rod, one-level sleeve, two-level sleeve, three-level sleeve, sealing
Circle and acoustic emission sensor are coaxially disposed, wherein:Ladder screw thread waveguide rod is provided with the first external screw thread, the second external screw thread, outside first
Screw thread is connected with the internal thread of one-level sleeve, so that the front end of ladder screw thread waveguide rod is placed in the first cavity of one-level sleeve and
In two cavitys, the second external screw thread is placed on the outside of the second cavity of one-level sleeve;Arrange in the rear end of ladder screw thread waveguide rod and fix
End, arranges the acoustic emission sensor being in contact with it in fixing end;One-level sleeve external screw thread is connected with three-level internal thread of sleeve, with
One-level sleeve is made to be placed in the 3rd cavity and the 4th cavity of three-level sleeve;Two-level sleeve is sleeved on the outside of three-level sleeve, two
Between level sleeve and three-level sleeve, sealing ring is set.
In above-mentioned technical proposal, the sealing ring is rubber seal.
In above-mentioned technical proposal, a diameter of 5 ± 0.01mm of the test surfaces of sample, length are 7~8mm.
In above-mentioned technical proposal, ladder screw thread waveguide rod and fixing end are metal material, such as ferritic stainless steel.
In above-mentioned technical proposal, one-level sleeve, two-level sleeve, three-level sleeve are insulating materials, such as polytetrafluoroethyl-ne
Alkene.
In above-mentioned technical proposal, adhesive phase is set between fixing end and acoustic emission sensor.
In above-mentioned technical proposal, acoustic emission sensor is fixed in fixing end using magnetic clamp.
When being used, ladder screw thread the second external screw thread of waveguide rod is connected with the internal thread of sample, in the periphery of sample
Coupling oxidant layer is set, the fixing end of ladder screw thread waveguide rod is rotated, so as to be connected with ladder screw thread the second external screw thread of waveguide rod
The test surfaces of sample, it is concordant with the second alignment surface of the first alignment surface of one-level sleeve, three-level sleeve;Using in second sleeve
Screw thread is fixedly linked with test device, and carries out electrochemical corrosion test to sample, with sample as working electrode, using wire with
Ladder screw thread waveguide rod on the outside of test device is connected, to gather the electrochemical corrosion signal on sample;Sample is in corrosion
During the sound emission elastic wave that sends acoustic emission sensor is reached by ladder screw thread waveguide rod and displacement signal is converted into
Electric signal, outwards transmits.
A kind of corrosion electrochemical test system, including electrolytic cell, electrochemical testing device, heater and attemperator;
The electrolytic cell includes reaction tank, reaction tank lid, gasket seal, fastener, sample erecting device, the reaction
Pond is cylinder, and reaction tank upper end-face edge is provided with flange, is lined with gasket seal at the top of the reaction tank lid and reaction tank, reacts
Chi Gai and the logical fastener sealing of reaction tank;Air inlet pipe thread hole, exhaust pipe thread hole, auxiliary electrode spiral shell are set on reaction tank lid
Pit, digital display thermometer probe screwed hole, Luggin capillary screwed hole;Air inlet pipe thread hole is connected with air inlet pipe, blast pipe spiral shell
Pit is connected with blast pipe, and auxiliary electrode screwed hole is connected with described auxiliary electrode, digital display thermometer probe screwed hole and number
Aobvious thermometer connection;Luggin capillary screwed hole is connected with the external screw thread of Luggin capillary liquid injection port, so that Luggin capillary
Crooked position in reaction tank, just to the sample as working electrode at its opening, the internal thread of Luggin capillary liquid injection port with
Reference electrode external screw thread is connected, so that reference liquid can be flow at the opening of sample in reference electrode;Luggin capillary
At opening, as working electrode sample and auxiliary electrode be located at same level on;Described sample erecting device is by rank
Ladder shell ripple guide rod, one-level sleeve, two-level sleeve, three-level sleeve, sealing ring composition, ladder screw thread waveguide rod, one-level sleeve, two
Level sleeve, three-level sleeve and sealing ring are coaxially disposed, wherein:Ladder screw thread waveguide rod is provided with the first external screw thread, the second external screw thread,
In the rear end of ladder screw thread waveguide rod, fixing end is set;First external screw thread is connected with the internal thread of one-level sleeve, so that ladder spiral shell
The front end of ripple guide rod is placed in first cavity and the second cavity of one-level sleeve, and the second external screw thread is placed in the second of one-level sleeve
On the outside of cavity;One-level sleeve external screw thread is connected with three-level internal thread of sleeve so that one-level sleeve be placed in three-level sleeve it is the 3rd empty
In chamber and the 4th cavity;Two-level sleeve is sleeved on the outside of three-level sleeve, between two-level sleeve and three-level sleeve arranges sealing ring;
The electrochemical testing device includes auxiliary electrode chuck, reference electrode chuck, working electrode chuck, electrochemistry number
According to processing system;The auxiliary electrode chuck, reference electrode chuck and working electrode chuck are electric with the auxiliary on electrolytic cell respectively
The fixing end of pole, reference electrode and ladder screw thread waveguide rod is connected, and is then processed with electrochemical data by signal transmssion line
System is connected;
Described heater is arranged on the outside of reaction tank, and attemperator is arranged on the outside of heater, heating dress
The inwall put arranges temperature sensor, for detecting the temperature change of electrolyte in reaction tank.
In above-mentioned technical proposal, the quantity of the fastener is 6~8 groups, and fastener is by " bow " shape fastener
Chuck, trip bolt and fastening gasket composition, fastener chuck material are 316 austenitic stainless steels;Fastener chuck bag
First level section, vertical section and the second horizontal segment are included, the second horizontal segment upper surface is provided with the thick fastening gasket for 2~3mm, tightly
Be fixedly mounted with put pad material be polytetrafluoroethylene (PTFE), to prevent fastening force from causing greatly very much aquarium to rupture.
In above-mentioned technical proposal, on described reaction tank lid, stainless steel locating ring is provided with, on the stainless steel locating ring
6~8 trip bolt locating slots are evenly distributed with, a diameter of 4~5mm of trip bolt locating slot, depth are 0.5~0.6mm, tightly
Gu screw locating slot is used to position described trip bolt, another effect of the stainless steel locating ring is subject to trip bolt
The fastening force of applying, it is to avoid the reaction tank lid is damaged by the trip bolt.
In above-mentioned technical proposal, described air inlet pipe thread hole quantity is 3~4, exhaust pipe thread hole quantity is 1~
2, Luggin capillary screw thread hole number is 1, and auxiliary electrode screw thread hole number is 1, digital display thermometer probe screw thread hole count
Measure as 1~2;Correspondingly, air inlet pipe quantity is 3~4, and blast pipe quantity is 1~2, and Luggin capillary quantity is 1,
Auxiliary electrode quantity is 1, and digital display thermometer probe quantity is 1~2;Air inlet pipe, blast pipe, Luggin capillary, auxiliary electricity
Pole and digital display thermometer probe respectively at air inlet pipe thread hole, exhaust pipe thread hole, Luggin capillary screwed hole, auxiliary electrode
Screwed hole, digital display thermometer probe screwed hole connect.
In above-mentioned technical proposal, described air inlet pipe and blast pipe are with externally threaded glass tube;The air inlet pipe
One end is equipped with for the scattered porous foam of bubble, it is therefore an objective to the dissolving for disperseing Input gas and accelerating which in corrosive medium;
The air inlet pipe be passed through high pure nitrogen or carbon dioxide or hydrogen sulfide in one kind, high pure nitrogen to corrosive medium deoxygenation,
Carbon dioxide, sulfuration can simulate actual corrosive environment;The air inlet pipe thread hole not used arranges sealing screw and is sealed,
The material of sealing screw is polytetrafluoroethylene (PTFE).
In above-mentioned technical proposal, described auxiliary electrode is gauze platinum electrode;Described reference electrode is arranged on Lu Jinmao
In tubule, the liquid injection port of the Luggin capillary is the structure with inside and outside double thread, the Luggin capillary external screw thread and institute
The Luggin capillary screwed hole connection on aquarium is stated, the Shandong gold capillary tube internal thread is led to the external screw thread of the reference electrode
Helicitic texture connection is crossed, and adopts rubber seal rings for seal;Registration coupon test surfaces at the opening at the Luggin capillary tip
The center of mouth, and the distance of 0.5~1mm is kept with tested sample.
In above-mentioned technical proposal, described temperature sensor quantity is 1~8;Described heater adopts resistance
Heated water bath or oil bath mode are heated to electrolytic cell, temperature sensor by closed-loop policy automatically control firing rate and water or
The temperature of oil, in the water that the reaction tank is put in heating and heat-insulating device or oil, the water level or oil level in heater is less than
Ladder screw thread waveguide rod 2~5cm of lower end;In heater and attemperator, by arranging heating target temperature, firing rate
Water or oil in the heater is heated, to be heated to after target temperature, heater stop heating, and ensure to add
Water or oil in thermal maintains target temperature ± 0.1 DEG C all the time.
In above-mentioned technical proposal, a diameter of 5 ± 0.01mm of the test surfaces of sample, length are 7~8mm.
In above-mentioned technical proposal, ladder screw thread waveguide rod be metal material, such as ferritic stainless steel;One-level sleeve,
Two-level sleeve, three-level sleeve are insulating materials, such as polytetrafluoroethylene (PTFE).
In above-mentioned technical proposal, the sealing ring is rubber seal.
When a kind of corrosion electrochemical test system is used, the internal thread of the second external screw thread of ladder screw thread waveguide rod and sample
Connection, sample periphery arrange coupling oxidant layer, rotate ladder screw thread waveguide rod fixing end so that with ladder screw thread waveguide
The test surfaces of the sample that the second external screw thread of bar is connected, the second alignment surface of the first alignment surface, three-level sleeve with one-level sleeve are put down
Together;It is fixedly linked using the internal thread and test device of second sleeve, and electrochemical corrosion test is carried out to sample, with sample is
Working electrode, is connected with the ladder screw thread waveguide rod on the outside of test device using wire, to gather the electrochemistry on sample
Corrosion signal;Digital display thermometer is popped one's head in and temperature sensor detects the true temperature of electrolytic cell internal corrosion medium, test to be achieved
Require temperature and test can be started after keeping stablizing.
A kind of electrochemical testing device of acoustic emission detection material corrosion performance, including electrolytic cell, electrochemical testing device,
Heater and attemperator;
The electrolytic cell includes reaction tank, reaction tank lid, gasket seal, fastener, sample erecting device, the reaction
Pond is cylinder, and reaction tank upper end-face edge is provided with flange, is lined with gasket seal at the top of the reaction tank lid and reaction tank, reacts
Chi Gai and the logical fastener sealing of reaction tank;Air inlet pipe thread hole, exhaust pipe thread hole, auxiliary electrode spiral shell are set on reaction tank lid
Pit, digital display thermometer probe screwed hole, Luggin capillary screwed hole;Air inlet pipe thread hole is connected with air inlet pipe, blast pipe spiral shell
Pit is connected with blast pipe, and auxiliary electrode screwed hole is connected with described auxiliary electrode, digital display thermometer probe screwed hole and number
Aobvious thermometer connection;Luggin capillary screwed hole is connected with the external screw thread of Luggin capillary liquid injection port, so that Luggin capillary
Crooked position in reaction tank, just to the sample as working electrode at its opening, the internal thread of Luggin capillary liquid injection port with
Reference electrode external screw thread is connected, so that reference liquid can be flow at the opening of sample in reference electrode;Luggin capillary
At opening, as working electrode sample and auxiliary electrode be located at same level on;Described sample erecting device is by rank
Ladder shell ripple guide rod, one-level sleeve, two-level sleeve, three-level sleeve, sealing ring and acoustic emission sensor composition, ladder screw thread waveguide
Bar, one-level sleeve, two-level sleeve, three-level sleeve, sealing ring and acoustic emission sensor are coaxially disposed, wherein:Ladder screw thread waveguide
Bar is provided with the first external screw thread, the second external screw thread, and the first external screw thread is connected with the internal thread of one-level sleeve, so that ladder screw thread waveguide
The front end of bar is placed in first cavity and the second cavity of one-level sleeve, and the second external screw thread is placed in outside the second cavity of one-level sleeve
Side;Fixing end is set in the rear end of ladder screw thread waveguide rod, the acoustic emission sensor being in contact with it is set in fixing end;One-level
Sleeve external screw thread is connected with three-level internal thread of sleeve, so that one-level sleeve is placed in the 3rd cavity and the 4th cavity of three-level sleeve
It is interior;Two-level sleeve is sleeved on the outside of three-level sleeve, between two-level sleeve and three-level sleeve arranges sealing ring;
The electrochemical testing device includes auxiliary electrode chuck, reference electrode chuck, working electrode chuck, electrochemistry number
According to processing system;The auxiliary electrode chuck, reference electrode chuck and working electrode chuck are electric with the auxiliary on electrolytic cell respectively
Pole, reference electrode and ladder screw thread waveguide rod are connected, and are then connected with electrochemical data processing system by signal transmssion line;
Described heater is arranged on the outside of reaction tank, and attemperator is arranged on the outside of heater, heating dress
The inwall put arranges temperature sensor, for detecting the temperature change of electrolyte in reaction tank.
In above-mentioned technical proposal, the quantity of the fastener is 6~8 groups, and fastener is by " bow " shape fastener
Chuck, trip bolt and fastening gasket composition, fastener chuck material are 316 austenitic stainless steels;Fastener chuck bag
First level section, vertical section and the second horizontal segment are included, the second horizontal segment upper surface is provided with the thick fastening gasket for 2~3mm, tightly
Be fixedly mounted with put pad material be polytetrafluoroethylene (PTFE), to prevent fastening force from causing greatly very much aquarium to rupture.
In above-mentioned technical proposal, on described reaction tank lid, stainless steel locating ring is provided with, on the stainless steel locating ring
6~8 trip bolt locating slots are evenly distributed with, a diameter of 4~5mm of trip bolt locating slot, depth are 0.5~0.6mm, tightly
Gu screw locating slot is used to position described trip bolt, another effect of the stainless steel locating ring is subject to trip bolt
The fastening force of applying, it is to avoid the reaction tank lid is damaged by the trip bolt.
In above-mentioned technical proposal, described air inlet pipe thread hole quantity is 3~4, exhaust pipe thread hole quantity is 1~
2, Luggin capillary screw thread hole number is 1, and auxiliary electrode screw thread hole number is 1, digital display thermometer probe screw thread hole count
Measure as 1~2;Correspondingly, air inlet pipe quantity is 3~4, and blast pipe quantity is 1~2, and Luggin capillary quantity is 1,
Auxiliary electrode quantity is 1, and digital display thermometer probe quantity is 1~2;Air inlet pipe, blast pipe, Luggin capillary, auxiliary electricity
Pole and digital display thermometer probe respectively at air inlet pipe thread hole, exhaust pipe thread hole, Luggin capillary screwed hole, auxiliary electrode
Screwed hole, digital display thermometer probe screwed hole connect.
In above-mentioned technical proposal, described air inlet pipe and blast pipe are with externally threaded glass tube;The air inlet pipe
One end is equipped with for the scattered porous foam of bubble, it is therefore an objective to the dissolving for disperseing Input gas and accelerating which in corrosive medium;
The air inlet pipe be passed through high pure nitrogen or carbon dioxide or hydrogen sulfide in one kind, high pure nitrogen to corrosive medium deoxygenation,
Carbon dioxide, sulfuration can simulate actual corrosive environment;The air inlet pipe thread hole not used arranges sealing screw and is sealed,
The material of sealing screw is polytetrafluoroethylene (PTFE).
In above-mentioned technical proposal, described auxiliary electrode is gauze platinum electrode;Described reference electrode is arranged on Lu Jinmao
In tubule, the liquid injection port of the Luggin capillary is the structure with inside and outside double thread, the Luggin capillary external screw thread and institute
The Luggin capillary screwed hole connection on aquarium is stated, the Shandong gold capillary tube internal thread is led to the external screw thread of the reference electrode
Helicitic texture connection is crossed, and adopts rubber seal rings for seal;Registration coupon test surfaces at the opening at the Luggin capillary tip
The center of mouth, and the distance of 0.5~1mm is kept with tested sample.
In above-mentioned technical proposal, described temperature sensor quantity is 1~8;Described heater adopts resistance
Heated water bath or oil bath mode are heated to electrolytic cell, temperature sensor by closed-loop policy automatically control firing rate and water or
The temperature of oil, in the water that the reaction tank is put in heating and heat-insulating device or oil, the water level or oil level in heater is less than
Ladder screw thread waveguide rod 2~5cm of lower end;In heater and attemperator, by arranging heating target temperature, firing rate
Water or oil in the heater is heated, to be heated to after target temperature, heater stop heating, and ensure to add
Water or oil in thermal maintains target temperature ± 0.1 DEG C all the time.
In above-mentioned technical proposal, a diameter of 5 ± 0.01mm of the test surfaces of sample, length are 7~8mm.
In above-mentioned technical proposal, ladder screw thread waveguide rod be metal material, such as ferritic stainless steel;One-level sleeve,
Two-level sleeve, three-level sleeve are insulating materials, such as polytetrafluoroethylene (PTFE).
In above-mentioned technical proposal, the sealing ring is rubber seal.
In above-mentioned technical proposal, adhesive phase is set between fixing end and acoustic emission sensor.
In above-mentioned technical proposal, acoustic emission sensor is fixed in fixing end using magnetic clamp.
When a kind of electrochemical testing device of acoustic emission detection material corrosion performance is used, outside ladder screw thread waveguide rod second
Screw thread is connected with the internal thread of sample, is arranged coupling oxidant layer in the periphery of sample, is rotated the fixing end of ladder screw thread waveguide rod,
So that the test surfaces of the sample being connected with ladder screw thread the second external screw thread of waveguide rod, the first alignment surface, three-level with one-level sleeve
Second alignment surface of sleeve is concordant;It is fixedly linked using the internal thread and test device of second sleeve, and electrification is carried out to sample
Corrosion test is learned, with sample as working electrode, is connected with the ladder screw thread waveguide rod on the outside of test device using wire, with
Electrochemical corrosion signal on collection sample;The sound emission elastic wave that sample is sent in corrosion process passes through ladder screw thread waveguide
Bar reaches acoustic emission sensor and displacement signal is converted into electric signal, outwards transmits;Digital display thermometer is popped one's head in and TEMP
Device coordinates the true temperature of detection electrolytic cell internal corrosion medium, test request temperature to be achieved holding start to survey after stablizing
Examination.
The invention has the advantages that:
1. sound emission Dynamic Non-Destruction Measurement technology and Electrochemical Measurement Technology are integrated by the present invention, realize it is online,
Dynamic, real-time detection material electrochemical corrosion process;The sample erecting device of the present invention is arranged in the side of aquarium, heating with
Attemperator can be heated to corrosive medium or is incubated by water-bath or oil bath mode.
2. the tested sample of the present invention is cylindrical tiny sample, the 19~20mm of area of test surfaces2, length is for only
7mm, can closely possible reduction damage of the sampling process to actual components.In addition, the present invention can realize it is micro- to actual components
The sampling at little position, such as welding point zones of different (root of weld, capping, Weld pipe mill, high temperature and low temperature heat affecting etc.).
3. the sample of the present invention is installed by the way of threaded connection, and transmits corrosion sound by ladder screw thread waveguide rod
Signal and electrochemical signals are penetrated, the mode conducted with wire with traditional epoxy sealing is compared, the tested sample of the present invention
Installation, dismounting, clean it is all more portable and efficient.
4. the present invention includes multiple air inlet pipe, can simulate material corrosion process under Various Complex corrosive gas environments;This
Invention secures the distance of Luggin capillary tip and tested sample, has unified the distance of Luggin capillary tip and tested sample
Impact to test result.
5. do not limited by checked object material, as long as conductive.
6. can use in severe complicated working condition, as long as operator's remote control under safety, suitable environment
, and detect that automatic degree is high, simple to operate, testing efficiency is higher, and labour intensity, testing equipment power consumption can be greatly reduced
It is low, it is easy to carry, it is easy to the detection of operation field.
Description of the drawings
Fig. 1 is the electrochemical testing device workflow diagram of the acoustic emission detection material corrosion performance of the present invention;
Fig. 2 is the electrolytic cell front view of the present invention;
Fig. 3 is the electrolytic cell side view of the present invention;
Fig. 4 is the electrolytic cell top view of the present invention;
Fig. 5 is the reaction tank schematic diagram of the present invention;
Fig. 6 is the fastener schematic diagram of the present invention;
Fig. 7 is the reaction tank lid schematic diagram of the present invention;
Fig. 8 is the sample erecting device schematic diagram a of the present invention;
Fig. 9 is the profile of Fig. 8;
Figure 10 is the ladder screw thread waveguide rod schematic diagram of the present invention;
Figure 11 is the one-level sleeve schematic diagram of the present invention;
Figure 12 is the two-level sleeve schematic diagram of the present invention;
Figure 13 is the three-level sleeve schematic diagram of the present invention;
Figure 14 is the sample schematic diagram and profile of the present invention;
Figure 15 is Luggin capillary scheme of installation of the present invention;
Figure 16 is the sample erecting device schematic diagram b of the present invention;
Wherein:1 fastener;2 reaction tank gasket seals;3 temperature sensors;4 heaters;5 attemperators;6 reactions
Chi Gai;7 reaction tanks;8 sample erecting devices;9 flanges;10 lateral external screw joints;
1-1 trip bolts, 1-2 first level sections, 1-3 vertical sections, 1-4 fastening gaskets, the second horizontal segments of 1-5;6-1 is fastened
Screw locating slot, 6-2 stainless steel locating rings, 6-3 air inlet pipe thread holes, 6-4 digital display thermometers probe screwed hole, 6-5 auxiliary electricity
Pole screwed hole, 6-6 Luggin capillary screwed holes, 6-7 exhaust pipe thread holes;6-6-1 reference electrodes, 6-6-2 Luggin capillaries, 6-
6-3 bends, at 6-6-4 openings;8-1 ladder screw thread waveguide rods, 8-2 fixing ends, 8-3 one-level sleeves, 8-4 two-level sleeves, 8-5
Three-level sleeve, 8-6 sealing rings, 8-7 samples, 8-8 acoustic emission sensors;The first external screw threads of 8-1-1, the second external screw threads of 8-1-2;8-
The first alignment surfaces of 3-1, the first cavitys of 8-3-2, the second cavitys of 8-3-3,8-3-4 sealing surfaces, 8-3-5 one-level sleeve external screw threads, 8-
3-6 one-level internal thread of sleeve;8-4-1 two-level sleeve internal threads;The second alignment surfaces of 8-5-1, the 3rd cavitys of 8-5-2,8-5-3 the 4th
Cavity, 8-5-4 three-level internal thread of sleeve;8-7-1 test surfaces, 8-7-2 sample peripheries, 8-7-3 sample internal threads.
Figure 17 is electrochemical corrosion polarization curve of the two phase stainless steel in the 1mol/L NaCl aqueous solution;
Figure 18 is electrochemical potentials of the two phase stainless steel in the 1mol/L NaCl aqueous solution, current density and testing time
Relation curve;
Figure 19 is sound emission amplitude of the two phase stainless steel in electrochemical corrosion course;
Figure 20 is acoustic emission count of the two phase stainless steel in electrochemical corrosion course;
Figure 21 is acoustic emission energy of the two phase stainless steel in electrochemical corrosion course;
Figure 22 is two phase stainless steel in the acoustic emission waveform (in Figure 18 1 point) during cathodic polarization;
Figure 23 is acoustic emission waveform (in Figure 18 2 point) of the two phase stainless steel in process of anodic polarization;
Figure 24 is acoustic emission waveform (in Figure 18 3 point) of the two phase stainless steel in process of anodic polarization;
Figure 25 is acoustic emission waveform (in Figure 18 4 point) of the two phase stainless steel in process of anodic polarization;
Figure 26 is acoustic emission waveform (in Figure 18 5 point) of the two phase stainless steel in process of anodic polarization;
Figure 27 is acoustic emission waveform (in Figure 18 6 point) of the two phase stainless steel in process of anodic polarization.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples, but should not be construed as the limit to the present invention
System.
For the sample erecting device in the sample clamp of electrochemical corrosion test, i.e. above-mentioned accompanying drawing 8, by ladder screw thread ripple
Guide rod, one-level sleeve, two-level sleeve, three-level sleeve and sealing ring composition, ladder screw thread waveguide rod, one-level sleeve, two-level sleeve,
Three-level sleeve and sealing ring are coaxially disposed, wherein:Ladder screw thread waveguide rod is provided with the first external screw thread, the second external screw thread, outside first
Screw thread is connected with the internal thread of one-level sleeve, so that the front end of ladder screw thread waveguide rod is placed in the first cavity of one-level sleeve and
In two cavitys, the second external screw thread is placed on the outside of the second cavity of one-level sleeve;Arrange in the rear end of ladder screw thread waveguide rod and fix
End;One-level sleeve external screw thread is connected with three-level internal thread of sleeve, so that one-level sleeve is placed in the 3rd cavity of three-level sleeve and
In four cavitys;Two-level sleeve is sleeved on the outside of three-level sleeve, between two-level sleeve and three-level sleeve arranges sealing ring.
In above-mentioned technical proposal, the sealing ring is rubber seal.
In above-mentioned technical proposal, a diameter of 5 ± 0.01mm of the test surfaces of sample, length are 7~8mm.
In above-mentioned technical proposal, ladder screw thread waveguide rod be metal material, such as ferritic stainless steel.
In above-mentioned technical proposal, one-level sleeve, two-level sleeve, three-level sleeve are insulating materials, such as polytetrafluoroethyl-ne
Alkene.
When being used, ladder screw thread the second external screw thread of waveguide rod is connected with the internal thread of sample, in the circumference of sample
Face arranges coupling oxidant layer, rotates the fixing end of ladder screw thread waveguide rod, so as to be connected with ladder screw thread the second external screw thread of waveguide rod
Sample test surfaces, it is concordant with the second alignment surface of the first alignment surface of one-level sleeve, three-level sleeve.Using second sleeve
Internal thread is fixedly linked with test device, and carries out electrochemical corrosion test to sample, with sample as working electrode, using wire
It is connected with the ladder screw thread waveguide rod on the outside of test device, to gather the electrochemical corrosion signal on sample.
Sample erecting device in the fixture of acoustic emission detection material corrosion performance, i.e. above-mentioned accompanying drawing 16, by ladder screw thread
Waveguide rod, one-level sleeve, two-level sleeve, three-level sleeve, sealing ring and acoustic emission sensor composition, ladder screw thread waveguide rod,
Level sleeve, two-level sleeve, three-level sleeve, sealing ring and acoustic emission sensor are coaxially disposed, wherein:Ladder screw thread waveguide rod is provided with
First external screw thread, the second external screw thread, the first external screw thread are connected with the internal thread of one-level sleeve, so that before ladder screw thread waveguide rod
End is placed in first cavity and the second cavity of one-level sleeve, and the second external screw thread is placed on the outside of the second cavity of one-level sleeve;
The rear end of ladder screw thread waveguide rod arranges fixing end, and the acoustic emission sensor being in contact with it is arranged in fixing end;One-level sleeve
External screw thread is connected with three-level internal thread of sleeve, so that one-level sleeve is placed in the 3rd cavity and the 4th cavity of three-level sleeve;Two
Level sleeve set arranges sealing ring on the outside of three-level sleeve between two-level sleeve and three-level sleeve.
In above-mentioned technical proposal, the sealing ring is rubber seal.
In above-mentioned technical proposal, a diameter of 5 ± 0.01mm of the test surfaces of sample, length are 7~8mm.
In above-mentioned technical proposal, ladder screw thread waveguide rod and fixing end are metal material, such as ferritic stainless steel.
In above-mentioned technical proposal, one-level sleeve, two-level sleeve, three-level sleeve are insulating materials, such as polytetrafluoroethyl-ne
Alkene.
In above-mentioned technical proposal, adhesive phase is set between fixing end and acoustic emission sensor.
In above-mentioned technical proposal, acoustic emission sensor is fixed in fixing end using magnetic clamp.
When being used, ladder screw thread the second external screw thread of waveguide rod is connected with the internal thread of sample, in the periphery of sample
Coupling oxidant layer is set, the fixing end of ladder screw thread waveguide rod is rotated, so as to be connected with ladder screw thread the second external screw thread of waveguide rod
The test surfaces of sample, it is concordant with the second alignment surface of the first alignment surface of one-level sleeve, three-level sleeve.Using in second sleeve
Screw thread is fixedly linked with test device, and carries out electrochemical corrosion test to sample, with sample as working electrode, using wire with
Ladder screw thread waveguide rod on the outside of test device is connected, to gather the electrochemical corrosion signal on sample;Sample is in corrosion
During the sound emission elastic wave that sends acoustic emission sensor is reached by ladder screw thread waveguide rod and displacement signal is converted into
Electric signal, outwards transmits.
A kind of corrosion electrochemical test system, including electrolytic cell, electrochemical testing device, heater and attemperator;
The electrolytic cell includes reaction tank, reaction tank lid, gasket seal, fastener, sample erecting device, and the reaction tank is cylinder
Shape, reaction tank upper end-face edge are provided with flange, are lined with gasket seal at the top of the reaction tank lid and reaction tank, reaction tank lid and anti-
Ying Chitong fasteners are sealed;Air inlet pipe thread hole, exhaust pipe thread hole, auxiliary electrode screwed hole, number are set on reaction tank lid
Aobvious thermometer probe screwed hole, Luggin capillary screwed hole;Air inlet pipe thread hole is connected with air inlet pipe, is vented pipe thread hole with row
Tracheae connects, and auxiliary electrode screwed hole be connected with described auxiliary electrode, and digital display thermometer is popped one's head in screwed hole and digital display thermometer
Connection;Luggin capillary screwed hole is connected with the external screw thread of Luggin capillary liquid injection port, so that the crooked position of Luggin capillary
In reaction tank, just to the sample as working electrode, the internal thread and reference electrode of Luggin capillary liquid injection port at its opening
External screw thread is connected, so that reference liquid can be flow at the opening of sample in reference electrode;At the opening of Luggin capillary, make
Sample and auxiliary electrode for working electrode is located in same level;Described sample erecting device is by ladder screw thread waveguide
Bar, one-level sleeve, two-level sleeve, three-level sleeve, sealing ring composition, ladder screw thread waveguide rod, one-level sleeve, two-level sleeve, three
Level sleeve and sealing ring are coaxially disposed, wherein:Ladder screw thread waveguide rod is provided with the first external screw thread, the second external screw thread, in ladder spiral shell
The rear end of ripple guide rod arranges fixing end;First external screw thread is connected with the internal thread of one-level sleeve, so that ladder screw thread waveguide rod
Front end be placed in first cavity and the second cavity of one-level sleeve, the second external screw thread is placed in outside the second cavity of one-level sleeve
Side;One-level sleeve external screw thread is connected with three-level internal thread of sleeve, so that one-level sleeve is placed in the 3rd cavity of three-level sleeve and
In four cavitys;Two-level sleeve is sleeved on the outside of three-level sleeve, between two-level sleeve and three-level sleeve arranges sealing ring;The electricity
Test chemical device includes auxiliary electrode chuck, reference electrode chuck, working electrode chuck, electrochemical data processing system;Institute
State auxiliary electrode chuck, reference electrode chuck and working electrode chuck respectively with electrolytic cell on auxiliary electrode, reference electrode with
And the fixing end of ladder screw thread waveguide rod is connected, and is then connected with electrochemical data processing system by signal transmssion line;It is described
Heater be arranged on the outside of reaction tank, attemperator is arranged on the outside of heater, and the inwall of heater is arranged
Temperature sensor, for detecting the temperature change of electrolyte in reaction tank.
In above-mentioned technical proposal, the quantity of the fastener is 6~8 groups, and fastener is by " bow " shape fastener
Chuck, trip bolt and fastening gasket composition, fastener chuck material are 316 austenitic stainless steels;Fastener chuck bag
First level section, vertical section and the second horizontal segment are included, the second horizontal segment upper surface is provided with the thick fastening gasket for 2~3mm, tightly
Be fixedly mounted with put pad material be polytetrafluoroethylene (PTFE), to prevent fastening force from causing greatly very much aquarium to rupture.
In above-mentioned technical proposal, on described reaction tank lid, stainless steel locating ring is provided with, on the stainless steel locating ring
6~8 trip bolt locating slots are evenly distributed with, a diameter of 4~5mm of trip bolt locating slot, depth are 0.5~0.6mm, tightly
Gu screw locating slot is used to position described trip bolt, another effect of the stainless steel locating ring is subject to trip bolt
The fastening force of applying, it is to avoid the reaction tank lid is damaged by the trip bolt.
In above-mentioned technical proposal, described air inlet pipe thread hole quantity is 3~4, exhaust pipe thread hole quantity is 1~
2, Luggin capillary screw thread hole number is 1, and auxiliary electrode screw thread hole number is 1, digital display thermometer probe screw thread hole count
Measure as 1~2;Correspondingly, air inlet pipe quantity is 3~4, and blast pipe quantity is 1~2, and Luggin capillary quantity is 1,
Auxiliary electrode quantity is 1, and digital display thermometer probe quantity is 1~2;Air inlet pipe, blast pipe, Luggin capillary, auxiliary electricity
Pole and digital display thermometer probe respectively at air inlet pipe thread hole, exhaust pipe thread hole, Luggin capillary screwed hole, auxiliary electrode
Screwed hole, digital display thermometer probe screwed hole connect.
In above-mentioned technical proposal, described air inlet pipe and blast pipe are with externally threaded glass tube;The air inlet pipe
One end is equipped with for the scattered porous foam of bubble, it is therefore an objective to the dissolving for disperseing Input gas and accelerating which in corrosive medium;
The air inlet pipe be passed through high pure nitrogen or carbon dioxide or hydrogen sulfide in one kind, high pure nitrogen to corrosive medium deoxygenation,
Carbon dioxide, sulfuration can simulate actual corrosive environment;The air inlet pipe thread hole not used arranges sealing screw and is sealed,
The material of sealing screw is polytetrafluoroethylene (PTFE);
In above-mentioned technical proposal, described auxiliary electrode is gauze platinum electrode;Described reference electrode is arranged on Lu Jinmao
In tubule, the liquid injection port of the Luggin capillary is the structure with inside and outside double thread, the Luggin capillary external screw thread and institute
The Luggin capillary screwed hole connection on aquarium is stated, the Shandong gold capillary tube internal thread is led to the external screw thread of the reference electrode
Helicitic texture connection is crossed, and adopts rubber seal rings for seal;Registration coupon test surfaces at the opening at the Luggin capillary tip
The center of mouth, and the distance of 0.5~1mm is kept with tested sample.
In above-mentioned technical proposal, described temperature sensor quantity is 1~8;Described heater adopts resistance
Heated water bath or oil bath mode are heated to electrolytic cell, temperature sensor by closed-loop policy automatically control firing rate and water or
The temperature of oil, in the water that the reaction tank is put in heating and heat-insulating device or oil, the water level or oil level in heater is less than
Ladder screw thread waveguide rod 2~5cm of lower end;In heater and attemperator, by arranging heating target temperature, firing rate
Water or oil in the heater is heated, to be heated to after target temperature, heater stop heating, and ensure to add
Water or oil in thermal maintains target temperature ± 0.1 DEG C all the time.
In above-mentioned technical proposal, a diameter of 5 ± 0.01mm of the test surfaces of sample, length are 7~8mm.
In above-mentioned technical proposal, ladder screw thread waveguide rod be metal material, such as ferritic stainless steel;One-level sleeve,
Two-level sleeve, three-level sleeve are insulating materials, such as polytetrafluoroethylene (PTFE).
In above-mentioned technical proposal, the sealing ring is rubber seal.
When a kind of corrosion electrochemical test system is used, the internal thread of the second external screw thread of ladder screw thread waveguide rod and sample
Connection, sample periphery arrange coupling oxidant layer, rotate ladder screw thread waveguide rod fixing end so that with ladder screw thread waveguide
The test surfaces of the sample that the second external screw thread of bar is connected, the second alignment surface of the first alignment surface, three-level sleeve with one-level sleeve are put down
Together;It is fixedly linked using the internal thread and test device of second sleeve, and electrochemical corrosion test is carried out to sample, with sample is
Working electrode, is connected with the ladder screw thread waveguide rod on the outside of test device using wire, to gather the electrochemistry on sample
Corrosion signal;Digital display thermometer is popped one's head in and temperature sensor detects the true temperature of electrolytic cell internal corrosion medium, test to be achieved
Require temperature and test can be started after keeping stablizing.
A kind of electrochemical testing device of acoustic emission detection material corrosion performance, including electrolytic cell, electrochemical testing device,
Heater and attemperator;The electrolytic cell includes that reaction tank, reaction tank lid, gasket seal, fastener, sample install dress
Put, the reaction tank is cylinder, reaction tank upper end-face edge is provided with flange, is lined with close at the top of the reaction tank lid and reaction tank
The logical fastener sealing of gasket, reaction tank lid and reaction tank;Air inlet pipe thread hole, exhaust pipe screw thread are set on reaction tank lid
Hole, auxiliary electrode screwed hole, digital display thermometer probe screwed hole, Luggin capillary screwed hole;Air inlet pipe thread hole and air inlet pipe
Connection, exhaust pipe thread hole are connected with blast pipe, and auxiliary electrode screwed hole is connected with described auxiliary electrode, and digital display thermometer is visited
Head thread hole is connected with digital display thermometer;Luggin capillary screwed hole is connected with the external screw thread of Luggin capillary liquid injection port, so that
The crooked position of Luggin capillary in reaction tank, just to the sample as working electrode, Luggin capillary fluid injection at its opening
The internal thread of mouth is connected with reference electrode external screw thread, so that reference liquid can be flow at the opening of sample in reference electrode;
At the opening of Luggin capillary, as working electrode sample and auxiliary electrode be located at same level on;Described sample
Erecting device is made up of ladder screw thread waveguide rod, one-level sleeve, two-level sleeve, three-level sleeve, sealing ring and acoustic emission sensor,
Ladder screw thread waveguide rod, one-level sleeve, two-level sleeve, three-level sleeve, sealing ring and acoustic emission sensor are coaxially disposed, wherein:
Ladder screw thread waveguide rod is provided with the first external screw thread, the second external screw thread, and the first external screw thread is connected with the internal thread of one-level sleeve, so that
The front end of ladder screw thread waveguide rod is placed in first cavity and the second cavity of one-level sleeve, and the second external screw thread is placed in one-level sleeve
The second cavity on the outside of;Fixing end is set in the rear end of ladder screw thread waveguide rod, the sound being in contact with it is set in fixing end and is sent out
Penetrate sensor;One-level sleeve external screw thread is connected with three-level internal thread of sleeve so that one-level sleeve be placed in three-level sleeve it is the 3rd empty
In chamber and the 4th cavity;Two-level sleeve is sleeved on the outside of three-level sleeve, between two-level sleeve and three-level sleeve arranges sealing ring;
The electrochemical testing device includes auxiliary electrode chuck, reference electrode chuck, working electrode chuck, electrochemical data processing system
System;The auxiliary electrode chuck, reference electrode chuck and working electrode chuck respectively with electrolytic cell on auxiliary electrode, reference electricity
Pole and ladder screw thread waveguide rod are connected, and are then connected with electrochemical data processing system by signal transmssion line;Described adds
Thermal is arranged on the outside of reaction tank, and attemperator is arranged on the outside of heater, and the inwall of heater arranges temperature
Sensor, for detecting the temperature change of electrolyte in reaction tank.
In above-mentioned technical proposal, the quantity of the fastener is 6~8 groups, and fastener is by " bow " shape fastener
Chuck, trip bolt and fastening gasket composition, fastener chuck material are 316 austenitic stainless steels;Fastener chuck bag
First level section, vertical section and the second horizontal segment are included, the second horizontal segment upper surface is provided with the thick fastening gasket for 2~3mm, tightly
Be fixedly mounted with put pad material be polytetrafluoroethylene (PTFE), to prevent fastening force from causing greatly very much aquarium to rupture.
In above-mentioned technical proposal, on described reaction tank lid, stainless steel locating ring is provided with, on the stainless steel locating ring
6~8 trip bolt locating slots are evenly distributed with, a diameter of 4~5mm of trip bolt locating slot, depth are 0.5~0.6mm, tightly
Gu screw locating slot is used to position described trip bolt, another effect of the stainless steel locating ring is subject to trip bolt
The fastening force of applying, it is to avoid the reaction tank lid is damaged by the trip bolt.
In above-mentioned technical proposal, described air inlet pipe thread hole quantity is 3~4, exhaust pipe thread hole quantity is 1~
2, Luggin capillary screw thread hole number is 1, and auxiliary electrode screw thread hole number is 1, digital display thermometer probe screw thread hole count
Measure as 1~2;Correspondingly, air inlet pipe quantity is 3~4, and blast pipe quantity is 1~2, and Luggin capillary quantity is 1,
Auxiliary electrode quantity is 1, and digital display thermometer probe quantity is 1~2;Air inlet pipe, blast pipe, Luggin capillary, auxiliary electricity
Pole and digital display thermometer probe respectively at air inlet pipe thread hole, exhaust pipe thread hole, Luggin capillary screwed hole, auxiliary electrode
Screwed hole, digital display thermometer probe screwed hole connect.
In above-mentioned technical proposal, described air inlet pipe and blast pipe are with externally threaded glass tube;The air inlet pipe
One end is equipped with for the scattered porous foam of bubble, it is therefore an objective to the dissolving for disperseing Input gas and accelerating which in corrosive medium;
The air inlet pipe be passed through high pure nitrogen or carbon dioxide or hydrogen sulfide in one kind, high pure nitrogen to corrosive medium deoxygenation,
Carbon dioxide, sulfuration can simulate actual corrosive environment;The air inlet pipe thread hole not used arranges sealing screw and is sealed,
The material of sealing screw is polytetrafluoroethylene (PTFE);
In above-mentioned technical proposal, described auxiliary electrode is gauze platinum electrode;Described reference electrode is arranged on Lu Jinmao
In tubule, the liquid injection port of the Luggin capillary is the structure with inside and outside double thread, the Luggin capillary external screw thread and institute
The Luggin capillary screwed hole connection on aquarium is stated, the Shandong gold capillary tube internal thread is led to the external screw thread of the reference electrode
Helicitic texture connection is crossed, and adopts rubber seal rings for seal;Registration coupon test surfaces at the opening at the Luggin capillary tip
The center of mouth, and the distance of 0.5~1mm is kept with tested sample.
In above-mentioned technical proposal, described temperature sensor quantity is 1~8;Described heater adopts resistance
Heated water bath or oil bath mode are heated to electrolytic cell, temperature sensor by closed-loop policy automatically control firing rate and water or
The temperature of oil, in the water that the reaction tank is put in heating and heat-insulating device or oil, the water level or oil level in heater is less than
Ladder screw thread waveguide rod 2~5cm of lower end;In heater and attemperator, by arranging heating target temperature, firing rate
Water or oil in the heater is heated, to be heated to after target temperature, heater stop heating, and ensure to add
Water or oil in thermal maintains target temperature ± 0.1 DEG C all the time.
In above-mentioned technical proposal, a diameter of 5 ± 0.01mm of the test surfaces of sample, length are 7~8mm.
In above-mentioned technical proposal, ladder screw thread waveguide rod be metal material, such as ferritic stainless steel;One-level sleeve,
Two-level sleeve, three-level sleeve are insulating materials, such as polytetrafluoroethylene (PTFE).
In above-mentioned technical proposal, the sealing ring is rubber seal.
In above-mentioned technical proposal, adhesive phase is set between fixing end and acoustic emission sensor.
In above-mentioned technical proposal, acoustic emission sensor is fixed in fixing end using magnetic clamp.
When a kind of electrochemical testing device of acoustic emission detection material corrosion performance is used, outside ladder screw thread waveguide rod second
Screw thread is connected with the internal thread of sample, is arranged coupling oxidant layer in the periphery of sample, is rotated the fixing end of ladder screw thread waveguide rod,
So that the test surfaces of the sample being connected with ladder screw thread the second external screw thread of waveguide rod, the first alignment surface, three-level with one-level sleeve
Second alignment surface of sleeve is concordant;It is fixedly linked using the internal thread and test device of second sleeve, and electrification is carried out to sample
Corrosion test is learned, with sample as working electrode, is connected with the ladder screw thread waveguide rod on the outside of test device using wire, with
Electrochemical corrosion signal on collection sample;The sound emission elastic wave that sample is sent in corrosion process passes through ladder screw thread waveguide
Bar reaches acoustic emission sensor and displacement signal is converted into electric signal, outwards transmits;Digital display thermometer is popped one's head in and TEMP
Device coordinates the true temperature of detection electrolytic cell internal corrosion medium, test request temperature to be achieved holding start to survey after stablizing
Examination.
Electrochemistry and acoustic emission detection are carried out using aforementioned four technical scheme composition test device, it is specific as follows:
The concrete structure of the reaction tank lid refers to Fig. 7, and 3 air inlet pipe (are not drawn in figure with 1 blast pipe
Go out) cover corresponding air inlet pipe thread hole and exhaust pipe thread hole connection respectively with the reaction tank, and adopt rubber seal
Sealing, air inlet pipe one end are packaged with for the scattered porous foam of bubble and are inserted into reaction tank bottom, and the other end passes through rubber
Pipe is connected with the gas cylinder of corresponding Input gas, and gas flow is controlled by flowmeter;Described blast pipe one end is slightly inserted into
In reaction tank, it is ensured that more than corrosive medium liquid level, the other end of the blast pipe is by rubber tube and equipped with alkali lye
5L sealing volumetric flask be connected, in volumetric flask equipped with enough sodium hydroxide lyes (3L) for absorb discharge sour gas
Body.All glass tubes adopt silica gel sealing with the interface of rubber tube.Saturation potassium chloride solution is filled using syringe
Then the reference electrode is passed through external screw thread and institute by the Luggin capillary, it is ensured that no bubble in the Luggin capillary
State Luggin capillary internal thread to be attached by helicitic texture, the reference electrode is calomel electrode, and reference liquid is saturation chlorine
Change aqueous solutions of potassium.The concrete structure of the sample erecting device refers to Fig. 8 and Fig. 9, outside the second of ladder screw thread waveguide rod
Appropriate vacuum grease is smeared on screw thread, to reduce corrosion acoustic emission signal decay, and rubber seal ladder screw thread ripple is enclosed within into
On second external screw thread of guide rod, the then a small amount of silica gel of uniform application, afterwards derotation on the sample periphery after mechanical polishing
The second external screw thread threaded connection of sample ladder screw thread waveguide rod, sample rotation is enough to after tight, start to rotate ladder spiral shell backward
The sample is slowly drawn in the one-level sleeve by ripple guide rod, until sample testing face and the first alignment surface, the second alignment surface
Be substantially parallel, the unnecessary silica gel being extruded then is wiped using dust-free paper, and sample testing face is repeatedly cleaned with alcohol, then
Sample erecting device is put into into 24h in drying box, after silica gel is fully cured, the rubber seal two grades of sets is enclosed within into
On cylinder, then the lateral external screw joint by whole sample erecting device by the two-level sleeve internal thread with reaction tank connects
Connect.
The etchant solution for having configured slowly is imported in the reaction tank, is to ensure that the sample testing face is completely immersed in corruption
Erosion solution in and do not spill over, it is desirable to inject reaction tank etchant solution volume be 1~1.4L.
The gasket seal of the reaction tank is enclosed within the reaction tank lid, is then put down gently on the reaction tank, adjusted
The direction of the reaction tank lid makes center of the Luggin capillary tip just to the sample testing face.
6 described fasteners are installed, the fastening gasket is close to the lower limb of the flange of reaction tank first, while
Trip bolt is directed at into the trip bolt locating slot on the stainless steel locating ring, institute is screwed successively using diagonal order then
6 fasteners stated.
Data collection and analysis software is opened, electro-chemical test parameter and sound emission acquisition parameter are set.The electrochemistry
The setting of test parameter includes electrochemical test method and corresponding test parameter, and such as potentiodynamic polarization need to arrange open circuit electricity
Position stabilization time, scanning potential range, potential scanning speed etc..The sound emission acquisition parameter is arranged includes that the signal amplifies
Device multiplication factor, threshold value, sample frequency, filter range, real-time display parameters etc..It should be noted that electro-chemical test ginseng
Number and sound emission acquisition parameter need according to specific sample material, corrosive environment, electrochemical test method and adjust;Then enter
Accurate acoustic emission sensor described in lead experimental evaluation and the Couplings of the ladder screw thread waveguide rod of breaking of rower.In the ladder spiral shell
Disconnected lead experiment is carried out on acoustic emission sensor installation end on ripple guide rod near the acoustic emission sensor, when collecting
Disconnected lead acoustic emission signal amplitude to think that the acoustic emission sensor and the ladder screw thread waveguide rod are coupled when being higher than 90dB good
It is good;Then, the gas cylinder valve of Input gas is opened, by flowmeter control input gas flow.
Finally, formally start experiment.To ensure as far as possible in experimentation quiet environment and avoid touch electrolytic cell and
Related connection line.After the completion of test, experiment will be automatically stopped.
Believed with the polarization curve during this device to test UNS S31803 two phase stainless steel potentiodynamic polarizations and sound emission
Number (electrochemical testing device:Gamry, Interface 1000, acoustic emission test device:PAC, PCI-2;Acoustic emission sensor
Model:R15A;Signal amplifier model:2/4/6-AST), the NaCl aqueous solution of the test solution for 1mol/L.By this device according to
After above-mentioned step is installed, opening described data collection and analysis software carries out the setting of experiment parameter.Heating target
Temperature setting is 60 DEG C.Electro-chemical test parameter setting:Electrochemical test method is potentiodynamic polarization, electric potential scanning scope for-
0.75 VSCE-0.6 VSCE, sweep speed is 0.5mVSCE/s, and OCP temperature-time is 30min, setting electric current density
Continue to exceed 100 μ A/cm2When, test is automatically stopped.Sound emission acquisition parameter is arranged:Signal amplifier multiplication factor is 40dB,
Threshold value is 30dB, and sample frequency is 2MSPS, and filter range is 20kHz-1MHz, and Real-time Collection parameter is amplitude, energy, meter
Number and waveform.
The valve of test front opening High Purity Nitrogen gas cylinder, controls high pure nitrogen with the flow velocity pair of 0.1mL/min by flowmeter
Test solution carries out deoxygenation, and the deoxygenation time is 1h.Meanwhile, click begins to warm up, until solution temperature is stable 60 in electrolytic cell
±0.1℃.Afterwards, click on and start testing button, test formally starts.Test result is as shown in Figure 17-27.
Figure 17 is electrochemical corrosion polarization curve of the two phase stainless steel in the 1mol/L NaCl aqueous solution (60 DEG C).Figure 17
Polarization curve is divided into Liang Ge branches:Cathodic polarization (as indicated with 1) and anode polarization (shown in 2,3,4,5,6).Cathodic polarization process
In it is main there is evolving hydrogen reaction, have bubble hydrogen to produce in specimen surface.Mainly there is the dissolving of metal, passivation in process of anodic polarization
Film is formed, passivating film dissolves etc..From the beginning of corrosion potential, with the rising of current potential, metal surface gradually forms passivating film, in office
Portion region passivating film can occur dissolving and produce sub- point corrosion pit, and the sub- point corrosion pit of formation is likely to repair due to being passivated again, such as
2 in Figure 17, shown in 3,4,5.When current potential exceedes pitting potential, due to the formation of stable point corrosion pit, current density can be drastically
Increase, as shown in Figure 17 6.
Figure 18 is electrochemical potentials of the two phase stainless steel in the 1mol/L NaCl aqueous solution (60 DEG C), current density and survey
The relation curve of examination time.
Figure 19 is sound emission amplitude of the two phase stainless steel in electrochemical corrosion course.In Figure 19,1,2,3,4,5,6 sound are sent out
Penetrate amplitude corresponding with current density with 1,2,3,4,5,6 polarization potentials in Figure 16 respectively.
Figure 20 and Figure 21 is respectively acoustic emission count and energy of the two phase stainless steel in electrochemical corrosion course.Bubble hydrogen
The sound emission that the acoustic emission signal amplitude of rupture generation, counting and energy form the generation of meta-stable points pit with passivation film rupture is believed
Number amplitude, count and energy is without significant difference.Compared with the acoustic emission signal that meta-stable points pit is produced, stable point corrosion pit is produced
Amplitude and the higher acoustic emission signal of energy, but count value significantly do not increase.
Figure 22-27 is distributed as acoustic emission waveform of the two phase stainless steel during potentiodynamic polarization, respectively correspond to Figure 17 or
In Figure 19 1,2,3,4,5,6.Burst hydrogen bubbles produce typical sudden acoustic emission signal, and local is passivated film rupture and shape
Mixed type acoustic emission signal is produced into point corrosion pit is stablized.This device can be realized completely while using acoustic emission and electrochemistry
The purpose of technical testing material corrosion performance.
Claims (9)
1. a kind of electrochemical testing device of acoustic emission detection material corrosion performance, it is characterised in that:Including electrolytic cell, electrochemistry
Test device, heater and attemperator;The electrolytic cell include reaction tank, reaction tank lid, gasket seal, fastener,
Sample erecting device, the reaction tank are cylinder, and reaction tank upper end-face edge is provided with flange, the reaction tank lid and reaction tank
Top is lined with gasket seal, reaction tank lid and the logical fastener sealing of reaction tank;Air inlet pipe thread hole, row are set on reaction tank lid
Gas-pipe thread hole, auxiliary electrode screwed hole, digital display thermometer probe screwed hole, Luggin capillary screwed hole;Air inlet pipe thread hole
It is connected with air inlet pipe, exhaust pipe thread hole is connected with blast pipe, and auxiliary electrode screwed hole is connected with described auxiliary electrode, digital display
Thermometer probe screwed hole is connected with digital display thermometer;The external screw thread phase of Luggin capillary screwed hole and Luggin capillary liquid injection port
Even, so that the crooked position of Luggin capillary is in reaction tank, just to the sample as working electrode, Shandong gold capillary at its opening
The internal thread of pipe liquid injection port is connected with reference electrode external screw thread, so that reference liquid can flow to opening for sample in reference electrode
At mouthful;At the opening of Luggin capillary, as working electrode sample and auxiliary electrode be located at same level on;Described
Sample erecting device is by ladder screw thread waveguide rod, one-level sleeve, two-level sleeve, three-level sleeve, sealing ring and acoustic emission sensor
Composition, ladder screw thread waveguide rod, one-level sleeve, two-level sleeve, three-level sleeve, sealing ring and acoustic emission sensor are coaxially disposed,
Wherein:Ladder screw thread waveguide rod is provided with the first external screw thread, the second external screw thread, and the first external screw thread is connected with the internal thread of one-level sleeve
Connect, so that the front end of ladder screw thread waveguide rod is placed in first cavity and the second cavity of one-level sleeve, the second external screw thread is placed in
On the outside of second cavity of one-level sleeve;Fixing end is set in the rear end of ladder screw thread waveguide rod, is arranged in fixing end and is connect with which
Tactile acoustic emission sensor;One-level sleeve external screw thread is connected with three-level internal thread of sleeve, so that one-level sleeve is placed in three-level sleeve
The 3rd cavity and the 4th cavity in;Two-level sleeve is sleeved on the outside of three-level sleeve, is set between two-level sleeve and three-level sleeve
Put sealing ring;The electrochemical testing device includes auxiliary electrode chuck, reference electrode chuck, working electrode chuck, electrochemistry
Data handling system, the auxiliary electrode chuck, reference electrode chuck and working electrode chuck respectively with electrolytic cell on auxiliary
Electrode, reference electrode and ladder screw thread waveguide rod are connected, then by signal transmssion line and electrochemical data processing system phase
Even;Described heater is arranged on the outside of reaction tank, and attemperator is arranged on the outside of heater, heater it is interior
Wall arranges temperature sensor, for detecting the temperature change of electrolyte in reaction tank.
2. the electrochemical testing device of a kind of acoustic emission detection material corrosion performance according to claim 1, its feature exist
In:The quantity of the fastener is 6~8 groups, and fastener is by " bow " shape fastener chuck, trip bolt and fastening gasket
Composition, fastener chuck material are 316 austenitic stainless steels;Fastener chuck includes first level section, vertical section and
Two horizontal segments, the second horizontal segment upper surface are provided with the thick fastening gasket for 2~3mm, and the material of fastener pad is poly- four
PVF, to prevent fastening force from causing greatly very much aquarium to rupture.
3. the electrochemical testing device of a kind of acoustic emission detection material corrosion performance according to claim 1, its feature exist
In:Stainless steel locating ring is provided with described reaction tank lid, 6~8 fastening spiral shells on the stainless steel locating ring, are evenly distributed with
Nail locating slot, a diameter of 4~5mm of trip bolt locating slot, it is deep be 0.5~0.6mm, trip bolt locating slot is used to position institute
The trip bolt stated, another effect of the stainless steel locating ring are subject to the fastening force of trip bolt applying, it is to avoid described
The reaction tank lid is damaged by trip bolt.
4. the electrochemical testing device of a kind of acoustic emission detection material corrosion performance according to claim 1, its feature exist
In:Described air inlet pipe thread hole quantity is 3~4, and exhaust pipe thread hole quantity is 1~2, Luggin capillary screw thread hole count
Measure as 1, auxiliary electrode screw thread hole number is 1, digital display thermometer probe screw thread hole number is 1~2;Correspondingly, air inlet
Pipe quantity is 3~4, and blast pipe quantity is 1~2, and Luggin capillary quantity is 1, and auxiliary electrode quantity is 1, digital display
Thermometer probe quantity is 1~2;Air inlet pipe, blast pipe, Luggin capillary, auxiliary electrode and digital display thermometer probe difference
In with air inlet pipe thread hole, exhaust pipe thread hole, Luggin capillary screwed hole, auxiliary electrode screwed hole, digital display thermometer probe
Screwed hole connects.
5. the electrochemical testing device of a kind of acoustic emission detection material corrosion performance according to claim 1, its feature exist
In:Described air inlet pipe and blast pipe are with externally threaded glass tube;Described air inlet pipe one end is equipped with scattered for bubble
Porous foam, it is therefore an objective to the dissolving for disperseing Input gas and accelerating which in corrosive medium;The air inlet pipe is passed through high pure nitrogen
Or carbon dioxide or the one kind in hydrogen sulfide, high pure nitrogen can simulate reality to corrosive medium deoxygenation, carbon dioxide, sulfuration
The corrosive environment on border;The air inlet pipe thread hole not used arranges sealing screw and is sealed, and the material of sealing screw is polytetrafluoro
Ethene.
6. the electrochemical testing device of a kind of acoustic emission detection material corrosion performance according to claim 1, its feature exist
In:Described auxiliary electrode is gauze platinum electrode;Described reference electrode is arranged in Luggin capillary, the Luggin capillary
Liquid injection port is the structure with inside and outside double thread, the Luggin capillary spiral shell on the Luggin capillary external screw thread and the aquarium
Pit connects, and the Shandong gold capillary tube internal thread is connected by helicitic texture with the external screw thread of the reference electrode, and adopts rubber
Glue sealing ring is sealed;The center of registration coupon test surfaces mouth at the opening at the Luggin capillary tip, and protect with tested sample
Hold the distance of 0.5~1mm.
7. the electrochemical testing device of a kind of acoustic emission detection material corrosion performance according to claim 1, its feature exist
In:Described temperature sensor quantity is 1~8;Described heater adopts resistance heating water-bath or oil bath mode to electricity
Xie Chi is heated, and temperature sensor automatically controls the temperature of firing rate and water or oil by closed-loop policy, by the reaction tank
In the water being put in heating and heat-insulating device or oil, the water level or oil level in heater less than ladder screw thread waveguide rod lower end 2~
5cm;In heater and attemperator, by arranging heating target temperature, firing rate to the water in the heater
It is or oil is heated, to be heated to after target temperature, heater stop heating, and ensure the water in heater or oil all the time
Maintain target temperature ± 0.1 DEG C.
8. the electrochemical testing device of a kind of acoustic emission detection material corrosion performance according to claim 1, its feature exist
In:A diameter of 5 ± 0.01mm of the test surfaces of sample, length are 7~8mm;Ladder screw thread waveguide rod be metal material, such as iron
Ferritic stainless steel;One-level sleeve, two-level sleeve, three-level sleeve are insulating materials, such as polytetrafluoroethylene (PTFE);The sealing ring is
Rubber seal;Adhesive phase is set between fixing end and acoustic emission sensor;Using magnetic clamp by acoustic emission sensor
It is fixed in fixing end.
9. a kind of electrochemical testing device of the acoustic emission detection material corrosion performance as described in claim 1~8 is in electrochemistry
Application in corrosion test, it is characterised in that:Ladder screw thread the second external screw thread of waveguide rod is connected with the internal thread of sample, in sample
Periphery arrange coupling oxidant layer, rotate ladder screw thread waveguide rod fixing end so that with the second outer spiral shell of ladder screw thread waveguide rod
The test surfaces of the sample that line is connected, it is concordant with the second alignment surface of the first alignment surface of one-level sleeve, three-level sleeve;Using second
The internal thread of sleeve is fixedly linked with test device, and carries out electrochemical corrosion test to sample, with sample as working electrode, profit
It is connected with the ladder screw thread waveguide rod on the outside of test device with wire, to gather the electrochemical corrosion signal on sample;Examination
The sound emission elastic wave that sample is sent in corrosion process reaches acoustic emission sensor by ladder screw thread waveguide rod and believes displacement
Number electric signal is converted into, is outwards transmitted;Digital display thermometer is popped one's head in and temperature sensor coordinates detection electrolytic cell internal corrosion medium
True temperature, test request temperature to be achieved holding can start test after stablizing.
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CN106932457A (en) * | 2017-04-20 | 2017-07-07 | 中国人民解放军理工大学 | A kind of system and electrolyte for anodic oxidation reactionses |
CN107561145A (en) * | 2017-07-13 | 2018-01-09 | 中国电力科学研究院 | Corrosion test chamber |
WO2019051896A1 (en) * | 2017-09-12 | 2019-03-21 | 北京工业大学 | Acoustic emission testing device and method adapted to surface of friction pair moving at high frequency |
CN111982644A (en) * | 2020-08-19 | 2020-11-24 | 中国特种设备检测研究院 | Device and method for manufacturing carbon steel pitting corrosion sample in situ by adopting electrochemical method |
CN112198202A (en) * | 2020-10-10 | 2021-01-08 | 杭州绿洁环境科技股份有限公司 | Electrochemical electrolytic cell |
CN113406132A (en) * | 2021-06-11 | 2021-09-17 | 太原科技大学 | In-situ observation method for morphology of non-metallic inclusions in ultra-pure non-oriented cold-rolled silicon steel |
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CN106932457A (en) * | 2017-04-20 | 2017-07-07 | 中国人民解放军理工大学 | A kind of system and electrolyte for anodic oxidation reactionses |
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CN107561145B (en) * | 2017-07-13 | 2021-03-02 | 中国电力科学研究院 | Corrosion test box |
WO2019051896A1 (en) * | 2017-09-12 | 2019-03-21 | 北京工业大学 | Acoustic emission testing device and method adapted to surface of friction pair moving at high frequency |
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CN111982644A (en) * | 2020-08-19 | 2020-11-24 | 中国特种设备检测研究院 | Device and method for manufacturing carbon steel pitting corrosion sample in situ by adopting electrochemical method |
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CN113406132A (en) * | 2021-06-11 | 2021-09-17 | 太原科技大学 | In-situ observation method for morphology of non-metallic inclusions in ultra-pure non-oriented cold-rolled silicon steel |
CN115683824A (en) * | 2022-11-14 | 2023-02-03 | 天津大学 | Fracture toughness testing arrangement of test piece under corrosive environment |
CN115683824B (en) * | 2022-11-14 | 2023-09-19 | 天津大学 | Fracture toughness testing device of test piece under corrosive environment |
CN117515382A (en) * | 2023-12-29 | 2024-02-06 | 中北大学 | Acoustic emission sensor clamp for laser cladding on-line monitoring |
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